#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/94/4319474.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4319474
loop_
_publ_author_name
'Julian Limburg'
'John S. Vrettos'
'Robert H. Crabtree'
'Gary W. Brudvig'
'Julio C. de Paula'
'Alia Hassan'
'Anne-Laure Barra'
'Carole Duboc-Toia'
'Marie-Noëlle Collomb'
_publ_section_title
;
 High-Frequency EPR Study of a New Mononuclear Manganese(III) Complex:
 [(terpy)Mn(N3)3] (terpy = 2,2':6',2''-Terpyridine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1698
_journal_page_last               1703
_journal_paper_doi               10.1021/ic001118j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C15 H11 N12 Mn '
_chemical_formula_sum            'C15 H11 Mn N12'
_chemical_formula_weight         414.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Tue Nov  8 12:05:09 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                93.79(1)
_cell_angle_beta                 103.17(1)
_cell_angle_gamma                103.11(1)
_cell_formula_units_Z            2
_cell_length_a                   8.481(1)
_cell_length_b                   8.907(2)
_cell_length_c                   12.109(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      18.1
_cell_measurement_theta_min      8.8
_cell_volume                     860.7(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.06169
_diffrn_orient_matrix_UB_12      -0.02231
_diffrn_orient_matrix_UB_13      0.07539
_diffrn_orient_matrix_UB_21      0.04346
_diffrn_orient_matrix_UB_22      0.11401
_diffrn_orient_matrix_UB_23      0.02567
_diffrn_orient_matrix_UB_31      -0.09970
_diffrn_orient_matrix_UB_32      -0.00038
_diffrn_orient_matrix_UB_33      0.03104
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  2.14
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3731
_diffrn_reflns_theta_max         26.28
_diffrn_standards_decay_%        -0.70
_diffrn_standards_interval_count 60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       plate
_exptl_crystal_F_000             420.00
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.079
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         2694
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0369
_refine_ls_shift/esd_max         0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0468
_reflns_number_observed          2694
_reflns_number_total             3486
_reflns_observed_criterion       3.00
_cod_data_source_file            ic001118j.cif
_cod_data_source_block           SRH315_BRUDVIG_-_LIMBURG
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 39 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        860.7(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C15 H11 N12 Mn '
_cod_database_code               4319474
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Mn 0.13335(5) 0.23337(5) 0.24100(4) 0.0226(1) Uani ? ?
N1 0.3528(3) 0.2745(3) 0.1641(2) 0.0250(6) Uani ? ?
N2 0.2180(3) 0.4767(3) 0.2513(2) 0.0222(6) Uani ? ?
N3 -0.0392(3) 0.3341(3) 0.3239(2) 0.0279(6) Uani ? ?
N4 -0.0184(3) 0.2197(3) 0.0895(2) 0.0322(7) Uani ? ?
N5 0.0223(3) 0.2923(3) 0.0156(2) 0.0313(7) Uani ? ?
N6 0.0542(4) 0.3585(4) -0.0577(3) 0.0561(10) Uani ? ?
N7 0.2937(3) 0.2436(3) 0.3908(2) 0.0346(7) Uani ? ?
N8 0.2704(4) 0.1559(3) 0.4580(2) 0.0435(8) Uani ? ?
N9 0.2518(6) 0.0773(5) 0.5271(3) 0.112(2) Uani ? ?
N10 0.0401(3) 0.0123(3) 0.2463(2) 0.0394(8) Uani ? ?
N11 -0.1018(3) -0.0508(3) 0.1958(2) 0.0346(7) Uani ? ?
N12 -0.2363(4) -0.1158(3) 0.1500(3) 0.0537(9) Uani ? ?
C1 0.4163(4) 0.1642(4) 0.1239(3) 0.0313(8) Uani ? ?
C2 0.5625(4) 0.1978(4) 0.0875(3) 0.0357(9) Uani ? ?
C3 0.6418(4) 0.3516(4) 0.0894(3) 0.0346(9) Uani ? ?
C4 0.5771(3) 0.4665(4) 0.1283(2) 0.0313(8) Uani ? ?
C5 0.4322(3) 0.4239(3) 0.1675(2) 0.0243(7) Uani ? ?
C6 0.3580(3) 0.5387(3) 0.2175(2) 0.0259(7) Uani ? ?
C7 0.4250(4) 0.6975(4) 0.2337(3) 0.0372(9) Uani ? ?
C8 0.3487(4) 0.7931(4) 0.2847(3) 0.0409(9) Uani ? ?
C9 0.2042(4) 0.7294(4) 0.3182(3) 0.0356(9) Uani ? ?
C10 0.1417(3) 0.5699(3) 0.2994(2) 0.0256(7) Uani ? ?
C11 -0.0106(3) 0.4896(3) 0.3340(2) 0.0269(7) Uani ? ?
C12 -0.1141(4) 0.5673(4) 0.3747(3) 0.0367(9) Uani ? ?
C13 -0.2510(4) 0.4800(5) 0.4064(3) 0.043(1) Uani ? ?
C14 -0.2798(4) 0.3215(5) 0.3971(3) 0.0416(10) Uani ? ?
C15 -0.1722(4) 0.2519(4) 0.3558(3) 0.0340(9) Uani ? ?
H1 0.357(4) 0.058(3) 0.120(2) 0.027(7) Uani ? ?
H2 0.606(4) 0.108(4) 0.059(3) 0.041(9) Uani ? ?
H3 0.739(4) 0.379(3) 0.070(2) 0.036(8) Uani ? ?
H4 0.633(4) 0.579(4) 0.133(3) 0.038(8) Uani ? ?
H5 0.513(5) 0.737(4) 0.205(3) 0.06(1) Uani ? ?
H6 0.395(4) 0.902(4) 0.303(3) 0.044(9) Uani ? ?
H7 0.156(4) 0.804(4) 0.362(3) 0.051(10) Uani ? ?
H8 -0.088(4) 0.681(4) 0.387(3) 0.045(9) Uani ? ?
H9 -0.329(4) 0.529(4) 0.440(3) 0.06(1) Uani ? ?
H10 -0.364(4) 0.266(4) 0.416(3) 0.038(9) Uani ? ?
H11 -0.186(4) 0.144(4) 0.345(2) 0.030(8) Uani ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 30 0.003 0.002 'International Tables'
H 0 22 0.000 0.000 'International Tables'
N 0 24 0.006 0.003 'International Tables'
Mn 0 2 0.337 0.728 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 MN N2 74.37(8) ? ? ? yes
N1 MN N3 148.30(9) ? ? ? yes
N1 MN N4 90.40(9) ? ? ? yes
N1 MN N7 87.37(9) ? ? ? yes
N1 MN N10 112.5(1) ? ? ? yes
N2 MN N3 73.93(8) ? ? ? yes
N2 MN N4 92.27(9) ? ? ? yes
N2 MN N7 88.37(9) ? ? ? yes
N2 MN N10 172.8(1) ? ? ? yes
N3 MN N4 90.61(9) ? ? ? yes
N3 MN N7 91.96(10) ? ? ? yes
N3 MN N10 99.2(1) ? ? ? yes
N4 MN N7 177.4(1) ? ? ? yes
N4 MN N10 90.1(1) ? ? ? yes
N7 MN N10 89.6(1) ? ? ? yes
MN N1 C1 125.5(2) ? ? ? yes
MN N1 C5 115.5(2) ? ? ? yes
C1 N1 C5 118.7(2) ? ? ? yes
MN N2 C6 119.6(2) ? ? ? yes
MN N2 C10 120.2(2) ? ? ? yes
C6 N2 C10 119.9(2) ? ? ? yes
MN N3 C11 115.5(2) ? ? ? yes
MN N3 C15 125.8(2) ? ? ? yes
C11 N3 C15 118.5(3) ? ? ? yes
MN N4 N5 122.4(2) ? ? ? yes
N4 N5 N6 177.0(3) ? ? ? yes
MN N7 N8 123.6(2) ? ? ? yes
N7 N8 N9 176.5(4) ? ? ? yes
MN N10 N11 120.9(2) ? ? ? yes
N10 N11 N12 177.3(3) ? ? ? yes
N1 C1 C2 122.6(3) ? ? ? yes
C1 C2 C3 118.3(3) ? ? ? yes
C2 C3 C4 120.0(3) ? ? ? yes
C3 C4 C5 118.6(3) ? ? ? yes
N1 C5 C4 121.7(3) ? ? ? yes
N1 C5 C6 115.4(2) ? ? ? yes
C4 C5 C6 122.9(3) ? ? ? yes
N2 C6 C5 114.9(2) ? ? ? yes
N2 C6 C7 120.6(3) ? ? ? yes
C5 C6 C7 124.5(3) ? ? ? yes
C6 C7 C8 119.6(3) ? ? ? yes
C7 C8 C9 119.7(3) ? ? ? yes
C8 C9 C10 118.4(3) ? ? ? yes
N2 C10 C9 121.7(3) ? ? ? yes
N2 C10 C11 115.5(2) ? ? ? yes
C9 C10 C11 122.8(3) ? ? ? yes
N3 C11 C10 114.4(2) ? ? ? yes
N3 C11 C12 122.2(3) ? ? ? yes
C10 C11 C12 123.4(3) ? ? ? yes
C11 C12 C13 118.2(3) ? ? ? yes
C12 C13 C14 119.7(3) ? ? ? yes
C13 C14 C15 118.9(3) ? ? ? yes
N3 C15 C14 122.4(3) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
MN N1 2.234(2) ? ? yes
MN N2 2.109(2) ? ? yes
MN N3 2.258(2) ? ? yes
MN N4 1.965(2) ? ? yes
MN N7 1.987(2) ? ? yes
MN N10 1.959(3) ? ? yes
N1 C1 1.337(4) ? ? yes
N1 C5 1.342(3) ? ? yes
N2 C6 1.355(3) ? ? yes
N2 C10 1.342(4) ? ? yes
N3 C11 1.343(4) ? ? yes
N3 C15 1.348(4) ? ? yes
N4 N5 1.206(3) ? ? yes
N5 N6 1.146(4) ? ? yes
N7 N8 1.182(3) ? ? yes
N8 N9 1.141(4) ? ? yes
N10 N11 1.204(3) ? ? yes
N11 N12 1.147(3) ? ? yes
C1 C2 1.385(4) ? ? yes
C2 C3 1.378(4) ? ? yes
C3 C4 1.371(4) ? ? yes
C4 C5 1.399(4) ? ? yes
C5 C6 1.480(4) ? ? yes
C6 C7 1.382(4) ? ? yes
C7 C8 1.373(5) ? ? yes
C8 C9 1.389(5) ? ? yes
C9 C10 1.382(4) ? ? yes
C10 C11 1.491(4) ? ? yes
C11 C12 1.385(4) ? ? yes
C12 C13 1.391(5) ? ? yes
C13 C14 1.369(5) ? ? yes
C14 C15 1.375(5) ? ? yes
